Phosphate homogeneous precipitant

Metal phosphates can be prepared by wet and dry methods. The homogeneous precipitation in aqueous systems is often employed to obtain uniformly sized and well-crystallized particles. The solid reactions can be used for preparation of some metal phosphates however, the particles with controlled morphology are difficult to synthesize. Moreover, the solid reaction consumes more energy than the reaction in aqueous system, except the hydrothermal reaction at elevated temperature. Recently the preparation from aqueous solution at low temperature received attention in view of saving energy and as an application for a wide variety of substances. Therefore the preparation of metal phosphate particles by the precipitation method is described next. Although phosphates include ortho-, pyro-, and polyphosphates, only orthophosphates are dealt with here. 

To control the size of the spherical aluminum phosphate particles, urea can be used as a homogeneous precipitation agent. The decomposition of urea at elevated temperatures plays an essential role in controlling the particles size. 

Spherical particles of various metal phosphate particles can be prepared by precipitation using urea as a homogeneous precipitation agent. Surface-active agents, such as SDS and CTAC, are effective in preparation of uniform-size spherical particles. The formed spherical particles are amorphous and contain OH- and H20, except cobalt phosphate particles with layered structure. These panicles are agglomerates of primary particles, and have pores of different sizes ranging from ultramicropore to mesopore. 

Anion or cation generation Anions can be generated slowly in solution to bring about homogeneous precipitation. Swift and Butler reviewed precipitation of the metal sulfides by use of thioacetamide or thiourea. PFHS of sulfides of cadmium, mercury, zinc, and nickel have been studied more recently by Swift and others. Phosphate can be generated by hydrolysis of triethyl phosphate, oxalate by hydrolysis of methyl oxalate, and sulfate by hydrolysis of diethyl sulfate or sulfamic acid. 

Delincee and Radola100 used a commercial preparation, as well as fresh tomatoes, for the preparation, purification, and characterization of tomato pectinesterase. The tomatoes were pressed and then homogenized directly with ammonium sulfate at 70% saturation. The precipitate obtained was extracted with 0.3 M phosphate and repeatedly salted out with ammonium sulfate, and the product was separated on a column of Sephadex G-75. The pattern of separation was similar to that in preceding work.50,97 A detailed study of the size properties of pectinesterase was conducted by gel-filtration and sedimentation analysis.100 By column and thin-layer gel-filtration on Sephadex G-75, the approximate molecular weight of a number of preparations of tomato pectinesterase was determined, values of 24,000 and 27,000 being obtained. A possible interaction of the... 

Because PMSE fails to inactivate acetylcholinesterase, this reagent is much less toxic than diisopropylfluoro-phosphate, and is also recommended as an alternative to the neurotoxic fluorophosphates and fluorophospho-nates. PMSE is freshly prepared as a 1-3 mM solution in water (higher concentrations will precipitate spontaneously). A better procedure is to first prepare a 20 mM PMSE solution in 2-propanol or dioxane this solution can then be added to the biological fluid with vortex mixing to achieve a 1-3 mM final concentration as a homogeneous solution. One should confirm that the alcohol or dioxane has little or no undesirable effect on enzymes or proteins of interest. See Chymotrypsin Protease Inhibitor Cocktails ... 

Precipitation of ferric hydroxide gel was also observed in the preparation of spindlelike hematite (a-Fe203) particles in a dilute ferric chloride solution in the presence of phosphate (9). In this case, however, the positive role of the gel was not definite since similar uniform hematite paricles were obtained as well in homogeneous systems in the presence of the same anions (9). Also, Hamada and Matijevic (10) prepared uniform particles of pseudocubic hematite by hydrolysis of ferric chloride in aqueous solutions of alcohol (10-50%) at I00°C for several days. In this reaction, it was observed that acicular crystals of (3-FeOOH precipitated first, and then they dissolved with formation of the pseudocubic particles of hematite. The intermediate P-FeOOH appears to work as a reservoir of the solute to maintain an ideal supersaturation for the nucleation and growth of the hematite. Since the (3-FeOOH as an intermediate and the pseudocubic shape tire not peculiar to the alcohol/water medium... 

The fish tissue sample containing AMO residues was homogenized with phosphate buffer (pH 4.5), followed by protein precipitation with TCA and SPE on a C18 cartridge. Trace amounts of nonpolar interfering substances present in the SPE eluate were removed by LLE using ether. The final extract was reacted with formaldehyde and TCA at 100°C for 30 min. A fluorescent derivative was extracted with ether three times, and the extracts were combined, evaporated, and reconstituted in the mobile phase. No interfering peaks from the control fish extract were observed. A proposed chemical structure of the fluorescent derivative was reported and confirmed by both MS and NMR experiments (73). 

The assay developed for this activity involves the reaction of the P5C with o-aminobenzaldehyde (OAB) to form the reaction product dihydroquinozoli-nium (DHQ). The DHQ and unreacted OAB were separated by reversed-phase HPLC (LiChrosorb C18). The column was eluted isocratically with a mobile phase of 1 part methanol to 2 parts water, and the separation shown in Figure 9.37 obtained. The reaction mixture contained L-omithine (35 mAf), a-ketoglutarate, potassium phosphate (pH 7.4), and pryidoxyl phosphate in a total volume of 2 mL. The reaction was started by the addition of the homogenate and terminated by the addition of 1 mL of 3 N HO containing the OAB. Precipitated protein was removed by centrifugation (3000 rpm), and samples of the supernatant solution (10 nL) were injected for analysis. 

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